Background technology
Novel lamellar stupalith Ti
2AlC has attracted lot of domestic and foreign scholar's exploration and research with its excellent properties.It had both had the performance of metal, can carry out traditional mechanical workout as having at normal temperatures under good electrical and thermal conductivity, lower Vickers' hardness, higher modulus of elasticity and shearing modulus, the room temperature, under comparatively high temps, had plasticity; This material has the performance of pottery again, like HMP, high thermal stability and good antioxidant property.But this material also exists sintering temperature high, and TR is little, and shortcoming such as hardness is low, strength ratio is less and limited its further application.
In recent years, for improving Ti
2The performance of AlC material, people utilize the means of solid solution highly malleablized and compoundization that it has been carried out study on the modification, have obtained effect preferably.Utilize the simple substance V element to carry out the solid solution study on the modification like document report (Scripta Materialia 53 (2005) 1369-1372); Its mechanical property is greatly improved; Can utilize the Zr element to carry out molten admittedly study on the modification with quadrat method; But this method raw materials cost is higher, and synthesis temperature is higher simultaneously, is unfavorable for its industrialization production; Also there is document (Scripta Materialia 50 (2004) 897-901) report to utilize Al
2O
3Particle can to Ti
2AlC has the Ti of analog structure
3AlC
2Material property carries out modification.But the present method that adopts is all more single, simultaneously, on the preparation method mainly with Al
2O
3And Ti
2Sintering is carried out in two kinds of powders mixing of AlC, perhaps with Al, C, TiO
2For raw material high temperature generates Ti through reduction reaction
2AlC/Al
2O
3Matrix material, but no matter the sort of technology all exists temperature of reaction high, and undercapacity, can't large-scale industrialized production.Patent (200910219290.8) has been reported and has been utilized high-energy ball milling to synthesize Ti
2AlC/Al
2O
3The novel method of matrix material, this method institute synthetic material is greatly improved on performance, but high-energy ball milling is difficult to suitability for industrialized production, simultaneously, matrix is not carried out the solid solution modification mutually.Therefore, how to take valid approach, utilize cheap material to synthesize Al
2O
3The solid solution type Ti of particle highly malleablized
2The AlC matrix material is a research emphasis from now on.
Summary of the invention
In order to overcome the defective of above-mentioned prior art, the object of the present invention is to provide a kind of (Ti, Zr)
2AlC/Al
2O
3Sosoloid matrix material and preparation method thereof utilizes Ti-Al-C-ZrO
2System is a raw material, prepares Al through thermite reaction reaction in technology low temperature
2O
3The Ti that strengthens
2AlC sosoloid matrix material; This method is utilized cheap oxide compound ZrO
2Substitute expensive metal simple-substance, reduced raw materials cost; Utilize the reaction heat of thermite reduction reaction self, reduced the synthesis temperature of material, simultaneously generated in-situ Al
2O
3The wild phase particle is tiny, even, and the performance of material is greatly improved; Prepared material has high-strength, fine and close, high temperature resistant, machinable performance characteristics.
In order to achieve the above object, technical scheme of the present invention is achieved in that
A kind of (Ti, Zr)
2AlC/Al
2O
3Sosoloid matrix material, its initial feed be purity more than or equal to 99%, fineness is smaller or equal to 200 purpose metal Ti powder, Al powder, C powder and MOX ZrO
2Carry out proportioning by following reaction formula:
2 (1-x) Ti+ (1+8x/3) Al+C+2xZrO
2→ (Ti
1-xZr
x)
2AlC+4x/3Al
2O
3(1) (x=0.005~0.2241), the result is Ti:39.38~70.08wt%, Al:20.11~22.85wt%, C:6.37~8.84wt%, ZrO
2: 0.97~31.41wt%.
The result is: a kind of (Ti, Zr)
2AlC/Al
2O
3The sosoloid matrix material, the raw material moity is: the Ti powder accounts for 39.38~70.08% of gross weight, and the Al powder accounts for 20.11~22.85% of gross weight, and the C powder accounts for 6.37~8.84% and ZrO of gross weight
2Powder accounts for 0.97~31.41% of gross weight.
A kind of (Ti, Zr)
2AlC/Al
2O
3The preparation technology of sosoloid matrix material the steps include:
Step 1, at first with purity more than or equal to 99%, fineness is smaller or equal to 200 purpose metal Ti powder, Al powder, C powder and MOX ZrO
2By following proportioning weighing, the Ti powder accounts for 39.38~70.08% of gross weight, and the Al powder accounts for 20.11~22.85% of gross weight, and the C powder accounts for 6.37~8.84% and ZrO of gross weight
2Powder accounts for 0.97~31.41% of gross weight;
Step 2, the batching in the step 1 is put into aluminum oxide ball milling jar on planetary ball mill, carry out mixing and ball milling; With the absolute ethyl alcohol is ball-milling medium; The rotating speed of ball mill is 600~900 rpms, material: ball: alcoholic acid mass ratio=1: 3: 1, ball milling 0.5~1.5 hour;
Step 3, the ball milling powder of step 2 gained is following dry 4~8 hours at 40~50 ℃;
Step 4, the dried powder of step 3 gained is packed in the graphite jig, under vacuum or argon gas condition, at 1100 ℃~1400 ℃, the pressure hot pressed sintering of 5.0~30MPa 1~2 hour;
Step 5, with step 4 gained material naturally cool to room temperature can obtain (Ti, Zr)
2AlC/Al
2O
3The sosoloid matrix material.
Institute of the present invention synthetic (Ti, Zr)
2AlC/Al
2O
3The sosoloid matrix material is characterized in that: it is made up of matrix phase and wild phase two portions, and matrix accounts for the 81.5-99.5% of matrix material gross weight mutually, and wild phase accounts for the 0.5-18.5% of gross weight, and matrix is (Ti mutually
1-x, Zr
x)
2AlC, wherein x gets 0.005~0.2241, and wild phase is Al
2O
3If Al in the matrix material that generates
2O
3Growing amount does not have enhancing, toughness reinforcing Ti less than 0.5% of product quality
2The effect of AlC matrix, otherwise, if Al in the product
2O
3Phasor surpasses Ti
2The content of AlC matrix phase can not be referred to as Ti
2The AlC based composites, simultaneously, Al
2O
3Growing amount will be above 18.5%, excessive Al
2O
3Not only do not have and improve Ti
2The effect of AlC can worsen its performance on the contrary.Therefore confirmed above compositional range.
The present invention utilizes Ti powder, Al powder, C powder and ZrO
2Powder is a raw material, through thermite reaction spontaneous particle wild phase Al in the process that matrix generates mutually
2O
3The metal simple-substance Zr that restores simultaneously is to Ti
2AlC carries out solution strengthening.Thereby prepared Al
2O
3The thin brilliant Ti of dispersion consolidatedization
2AlC sosoloid matrix material.Should be because this technology institute synthetic material composition adjustability be big, and firing temperature is low, even structure is fine and close, and cost is lower, and mechanical property is excellent, has widened the range of application of this matrix material.
Embodiment
Embodiment one
A kind of (Ti, Zr)
2AlC/Al
2O
3The sosoloid matrix material, its raw material weight moity is: 20.38%, the 1200 purpose C powder that 63.86%, the 200 purpose Al powder that 270 purpose Ti powder account for gross weight account for gross weight account for 8.15% and ZrO of gross weight
2Powder accounts for 7.61% of gross weight.
The step of preparation process of present embodiment is following:
Step 1, at first with purity more than or equal to 99%, fineness is smaller or equal to 200 purpose metal Ti powder, Al powder, C powder and MOX ZrO
2By following proportioning weighing, 20.38%, the 1200 purpose C powder that 63.86%, the 200 purpose Al powder that 270 purpose Ti powder account for gross weight account for gross weight account for gross weight 8.15%, ZrO
2Powder accounts for 7.61% of gross weight;
Step 2, the batching in the step 1 is put into aluminum oxide ball milling jar on planetary ball mill, carrying out mixing and ball milling, is ball-milling medium with the absolute ethyl alcohol, and the rotating speed of ball mill is 800 rpms, material: ball: alcoholic acid mass ratio=1: 3: 1, ball milling 1 hour;
Step 3, the ball milling powder of step 2 gained is following dry 6 hours at 44 ℃;
Step 4, the dried powder of step 3 gained is packed in the graphite jig, under vacuum or argon gas condition, at 1350 ℃, the pressure hot pressed sintering of 16MPa 2 hours;
Step 5, with step 4 gained material naturally cool to room temperature can obtain (Ti, Zr)
2AlC/Al
2O
3The sosoloid matrix material.
Present embodiment institute synthetic (Ti, Zr)
2AlC/Al
2O
3The sosoloid matrix material is characterized in that: it is made up of matrix phase and wild phase two portions, and matrix accounts for 96% of matrix material gross weight mutually, and wild phase accounts for 4% of gross weight, and matrix is (Ti mutually
0.9576, Zr
0.0424)
2AlC, wild phase are Al
2O
3
With reference to accompanying drawing, show this material matrix by (Ti, Zr)
2The AlC phase contains the TiC phase of small amount of impurities, and wild phase is Al
2O
3Phase.
Embodiment two
A kind of (Ti, Zr)
2AlC/Al
2O
3The sosoloid matrix material, its raw material weight moity is: 21.64%, the 1200 purpose C powder that 66.08%, the 200 purpose Al powder that 270 purpose Ti powder account for gross weight account for gross weight account for 8.46% and ZrO of gross weight
2Powder accounts for 3.82% of gross weight.
The step of preparation process of present embodiment is following:
Step 1, at first with purity more than or equal to 99%, fineness is smaller or equal to 200 purpose metal Ti powder, Al powder, C powder and MOX ZrO
2By following proportioning weighing, 21.64%, the 1200 purpose C powder that 66.08%, the 200 purpose Al powder that 270 purpose Ti powder account for gross weight account for gross weight account for gross weight 8.46%, ZrO
2Powder accounts for 3.82% of gross weight;
Step 2, the batching in the step 1 is put into aluminum oxide ball milling jar on planetary ball mill, carrying out mixing and ball milling, is ball-milling medium with the absolute ethyl alcohol, and the rotating speed of ball mill is 800 rpms, material: ball: alcoholic acid mass ratio=1: 3: 1, ball milling 1 hour;
Step 3, the ball milling powder of step 2 gained is following dry 6 hours at 47 ℃;
Step 4, the dried powder of step 3 gained is packed in the graphite jig, under vacuum or argon gas condition, at 1350 ℃, the pressure hot pressed sintering of 16MPa 2 hours;
Step 5, with step 4 gained material naturally cool to room temperature can obtain (Ti, Zr)
2AlC/Al
2O
3The sosoloid matrix material.
Present embodiment institute synthetic (Ti, Zr)
2AlC/Al
2O
3The sosoloid matrix material is characterized in that: it is made up of matrix phase and wild phase two portions, and matrix accounts for 98% of matrix material gross weight mutually, and wild phase accounts for 2% of gross weight, and matrix is (Ti mutually
0.9795, Zr
0.0205)
2AlC, wild phase are Al
2O
3
Embodiment three
A kind of (Ti, Zr)
2AlC/Al
2O
3The sosoloid matrix material, its raw material weight moity is: 21.04%, the 1200 purpose C powder that 54.56%, the 200 purpose Al powder that 270 purpose Ti powder account for gross weight account for gross weight account for 7.53% and ZrO of gross weight
2Powder accounts for 16.87% of gross weight.
The step of preparation process of present embodiment is following:
Step 1, at first with purity more than or equal to 99%, fineness is smaller or equal to 200 purpose metal Ti powder, Al powder, C powder and MOX ZrO
2By following proportioning weighing, 54.56%, the 200 purpose Al powder that 270 purpose Ti powder account for gross weight account for that 21.04%, 1200 purpose C powder account for 7.53%, ZrO
2Powder accounts for 16.87;
Step 2, the batching in the step 1 is put into aluminum oxide ball milling jar on planetary ball mill, carrying out mixing and ball milling, is ball-milling medium with the absolute ethyl alcohol, and the rotating speed of ball mill is 800 rpms, material: ball: alcoholic acid mass ratio=1: 3: 1, ball milling 1 hour;
Step 3, the ball milling powder of step 2 gained is following dry 6 hours at 44 ℃;
Step 4, the dried powder of step 3 gained is packed in the graphite jig, under vacuum or argon gas condition, at 1350 ℃, the pressure hot pressed sintering of 16MPa 2 hours;
Step 5, with step 4 gained material naturally cool to room temperature can obtain (Ti, Zr)
2AlC/Al
2O
3The sosoloid matrix material.
Present embodiment institute synthetic (Ti, Zr)
2AlC/Al
2O
3The sosoloid matrix material is characterized in that: it is made up of matrix phase and wild phase two portions, and matrix accounts for 92% of matrix material gross weight mutually, and wild phase accounts for 8% of gross weight, and matrix is (Ti mutually
0.9087, Zr
0.0913)
2AlC, wild phase are Al
2O
3